Deformation of two-phase aggregates with in situ X-ray tomography in rotating Paris-Edinburgh cell at GPa pressures and high temperature.

High-pressure (>1 GPa) torsion apparatus can be coupled with in situ X-ray tomography (XRT) to study microstructures in materials associated with large shear strains. Here, deformation experiments were carried out on multi-phase aggregates at ∼3-5 GPa and ∼300-500°C, using a rotational tomography Paris-Edinburgh press (RoToPEc) with in situ absorption contrast XRT on the PSICHE beamline at Synchrotron SOLEIL. The actual shear strain reached in the samples was quantified with respect to the anvil twisting angles, which is γ ≤ 1 at 90° anvil twist and reaches γ ≃ 5 at 225° anvil twist. 2D and 3D quantifications based on XRT that can be used to study in situ the deformation microfabrics of two-phase aggregates at high shear strain are explored. The current limitations for investigation in real time of deformation microstructures using coupled synchrotron XRT with the RoToPEc are outlined.

Femtosecond Visualization of hcp-Iron Strength and Plasticity under Shock Compression.

Iron is a key constituent of planets and an important technological material. Here, we combine in situ ultrafast x-ray diffraction with laser-induced shock compression experiments on Fe up to 187(10) GPa and 4070(285) K at 10^{8} s^{-1} in strain rate to study the plasticity of hexagonal-close-packed (hcp)-Fe under extreme loading states. {101[over ¯]2} deformation twinning controls the polycrystalline Fe microstructures and occurs within 1 ns, highlighting the fundamental role of twinning in hcp polycrystals deformation at high strain rates. The measured deviatoric stress initially increases to a significant elastic overshoot before the onset of flow, attributed to a slower defect nucleation and mobility. The initial yield strength of materials deformed at high strain rates is thus several times larger than their longer-term flow strength. These observations illustrate how time-resolved ultrafast studies can reveal distinctive plastic behavior in materials under extreme environments.

Deformation Behavior across the Zircon-Scheelite Phase Transition.

The pressure effects on plastic deformation and phase transformation mechanisms of materials are of great importance to both Earth science and technological applications. Zircon-type materials are abundant in both nature and the industrial field; however, there is still no in situ study of their deformation behavior. Here, by employing radial x-ray diffraction in a diamond anvil cell, we investigate the dislocation-induced texture evolution of zircon-type gadolinium vanadate (GdVO_{4}) in situ under pressure and across its phase transitions to its high-pressure polymorphs. Zircon-type GdVO_{4} develops a (001) compression texture associated with dominant slip along ⟨100⟩{001} starting from 5 GPa. This (001) texture transforms into a (110) texture during the zircon-scheelite phase transition. Our observation demonstrates a martensitic mechanism for the zircon-scheelite transformation. This work will help us understand the local deformation history in the upper mantle and transition zone and provides fundamental guidance on material design and processing for zircon-type materials.

Single-crystal diffraction at the Extreme Conditions beamline P02.2: procedure for collecting and analyzing high-pressure single-crystal data.

Fast detectors employed at third-generation synchrotrons have reduced collection times significantly and require the optimization of commercial as well as customized software packages for data reduction and analysis. In this paper a procedure to collect, process and analyze single-crystal data sets collected at high pressure at the Extreme Conditions beamline (P02.2) at PETRA III, DESY, is presented. A new data image format called `Esperanto' is introduced that is supported by the commercial software package CrysAlis(Pro) (Agilent Technologies UK Ltd). The new format acts as a vehicle to transform the most common area-detector data formats via a translator software. Such a conversion tool has been developed and converts tiff data collected on a Perkin Elmer detector, as well as data collected on a MAR345/555, to be imported into the CrysAlis(Pro) software. In order to demonstrate the validity of the new approach, a complete structure refinement of boron-mullite (Al5BO9) collected at a pressure of 19.4 (2) GPa is presented. Details pertaining to the data collections and refinements of B-mullite are presented.

X-ray Free Electron Laser-Induced Synthesis of ε-Iron Nitride at High Pressures.

The ultrafast synthesis of ε-Fe3N1+x in a diamond-anvil cell (DAC) from Fe and N2 under pressure was observed using serial exposures of an X-ray free electron laser (XFEL). When the sample at 5 GPa was irradiated by a pulse train separated by 443 ns, the estimated sample temperature at the delay time was above 1400 K, confirmed by in situ transformation of α- to γ-iron. Ultimately, the Fe and N2 reacted uniformly throughout the beam path to form Fe3N1.33, as deduced from its established equation of state (EOS). We thus demonstrate that the activation energy provided by intense X-ray exposures in an XFEL can be coupled with the source time structure to enable exploration of the time-dependence of reactions under high-pressure conditions.

In situ rheological measurements at extreme pressure and temperature using synchrotron X-ray diffraction and radiography.

Dramatic technical progress seen over the past decade now allows the plastic properties of materials to be investigated under extreme pressure and temperature conditions. Coupling of high-pressure apparatuses with synchrotron radiation significantly improves the quantification of differential stress and specimen textures from X-ray diffraction data, as well as specimen strains and strain rates by radiography. This contribution briefly reviews the recent developments in the field and describes state-of-the-art extreme-pressure deformation devices and analytical techniques available today. The focus here is on apparatuses promoting deformation at pressures largely in excess of 3 GPa, namely the diamond anvil cell, the deformation-DIA apparatus and the rotational Drickamer apparatus, as well as on the methods used to carry out controlled deformation experiments while quantifying X-ray data in terms of materials rheological parameters. It is shown that these new techniques open the new field of in situ investigation of materials rheology at extreme conditions, which already finds multiple fundamental applications in the understanding of the dynamics of Earth-like planet interior.

Kinetics and detectability of the bridgmanite to post-perovskite transformation in the Earth's D″ layer.

Bridgmanite, the dominant mineral in the Earth's lower mantle, crystallizes in the perovskite structure and transforms into post-perovskite at conditions relevant for the D[Formula: see text] layer. This transformation affects the dynamics of the Earth's lowermost mantle and can explain a range of seismic observations. The thickness over which the two phases coexist, however, can extend over 100 km, casting doubt on the assignment of the observed seismic boundaries. Here, experiments show that the bridgmanite to post-perovskite transition in (Mg[Formula: see text],Fe[Formula: see text])SiO[Formula: see text] is fast on geological timescales. The transformation kinetics, however, affects reflection coefficients of [Formula: see text] and [Formula: see text] waves by more than one order of magnitude. Thick layers of coexisting bridgmanite and post-perovskite can hence be detected using seismic reflections. Morever, the detection and wave period dependence of D[Formula: see text] reflections can be used to constrain significant features of the Earth's lowermost mantle, such as the thickness of the coexistence layer, and obtain information on temperature and grain sizes.

X-ray diffraction evaluation of stress in high pressure deformation experiments.

This paper explores the applicability of x-ray diffraction measurements of stress to high pressure deformation experiments. We model measurements of elastic lattice strains in various geometries for both axial and rotational deformation apparatus. We then show that, for most cases, stresses can be inverted from the diffraction data. A comparison between the results of our models and actual experimental data also indicates that plastic deformation can have an influence that is not addressed properly in the elastic models of lattice strains and should therefore be treated with caution.

Quantitative Rietveld texture analysis of CaSiO(3) perovskite deformed in a diamond anvil cell.

The Rietveld method is used to extract quantitative texture information from a single synchrotron diffraction image of a CaSiO(3) perovskite sample deformed in axial compression in a diamond anvil cell. The image used for analysis was taken in radial geometry at 49 GPa and room temperature. We obtain a preferred orientation of {100} lattice planes oriented perpendicular to the compression direction and this is compatible with [Formula: see text] slip.

Axial temperature gradient and stress measurements in the deformation-DIA cell using alumina pistons.

The deformation-DIA apparatus (D-DIA) coupled with synchrotron X-rays allows investigating materials elastic and plastic properties at high pressure. Most D-DIA deformation cells use alumina pistons that can also be used for measurement of the differential stress in the compression column by in situ X-ray diffraction. Here, we quantify the axial temperature (T) gradient in the D-DIA deformation cell and better constrain stress measurements in its compression column by studying an alumina specimen compressed and deformed at pressure P in the range 3.9-5.5 GPa and nominal temperature To = 1673 K. The axial T gradient, obtained from alumina equation of state, is ∼155 K∕mm at the centre of the cell and does not vary significantly during deformation to 20% specimen strain. This T gradient, if not taken into account when measuring the experimental pressure in the alumina pistons, leads to significantly overestimating pressure. Unlike pressure, stress measurements in alumina are weakly sensitive to temperature. During deformation, the "true" differential stress in the compression column is evaluated at 596 ± 20 MPa using an elastoplastic self-consistent model, while raw uncertainties on experimental differential stresses reach 84 MPa. A comparison between the simulated and experimental data allows to conclude that, although dislocation glide in the basal plane is the primary slip system at run condition, with an estimated critical resolved shear stress (CRSS) of 120 MPa, prism plane slips and pyramidal plane slips also contribute significantly to the aggregate homogenous deformation and texture development, with CRSS on the order of 280 MPa.

Experimental method for in situ determination of material textures at simultaneous high pressure and high temperature by means of radial diffraction in the diamond anvil cell.

We introduce the design and capabilities of a resistive heated diamond anvil cell that can be used for side diffraction at simultaneous high pressure and high temperature. The device can be used to study lattice-preferred orientations in polycrystalline samples up to temperatures of 1100 K and pressures of 36 GPa. Capabilities of the instrument are demonstrated with preliminary results on the development of textures in the bcc, fcc, and hcp polymorphs of iron during a nonhydrostatic compression experiment at simultaneous high pressure and high temperature.

High-pressure creep of serpentine, interseismic deformation, and initiation of subduction.

The supposed low viscosity of serpentine may strongly influence subduction-zone dynamics at all time scales, but until now its role could not be quantified because measurements relevant to intermediate-depth settings were lacking. Deformation experiments on the serpentine antigorite at high pressures and temperatures (1 to 4 gigapascals, 200 degrees to 500 degrees C) showed that the viscosity of serpentine is much lower than that of the major mantle-forming minerals. Regardless of the temperature, low-viscosity serpentinized mantle at the slab surface can localize deformation, impede stress buildup, and limit the downdip propagation of large earthquakes at subduction zones. Antigorite enables viscous relaxation with characteristic times comparable to those of long-term postseismic deformations after large earthquakes and slow earthquakes. Antigorite viscosity is sufficiently low to make serpentinized faults in the oceanic lithosphere a site for subduction initiation.

Deformation of (Mg,Fe)SiO3 post-perovskite and D'' anisotropy.

Polycrystalline (Mg(0.9),Fe(0.1))SiO3 post-perovskite was plastically deformed in the diamond anvil cell between 145 and 157 gigapascals. The lattice-preferred orientations obtained in the sample suggest that slip on planes near (100) and (110) dominate plastic deformation under these conditions. Assuming similar behavior at lower mantle conditions, we simulated plastic strains and the contribution of post-perovskite to anisotropy in the D'' region at the Earth core-mantle boundary using numerical convection and viscoplastic polycrystal plasticity models. We find a significant depth dependence of the anisotropy that only develops near and beyond the turning point of a downwelling slab. Our calculated anisotropies are strongly dependent on the choice of elastic moduli and remain hard to reconcile with seismic observations.

Plastic deformation of MgGeO3 post-perovskite at lower mantle pressures.

Polycrystalline MgGeO3 post-perovskite was plastically deformed in the diamond anvil cell between 104 and 130 gigapascals confining pressure and ambient temperature. In contrast with phenomenological considerations suggesting (010) as a slip plane, lattice planes near (100) became aligned perpendicular to the compression direction, suggesting that slip on (100) or (110) dominated plastic deformation. With the assumption that silicate post-perovskite behaves similarly at lower mantle conditions, a numerical model of seismic anisotropy in the D'' region implies a maximum contribution of post-perovskite to shear wave splitting of 3.7% with an oblique polarization.